HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Hydroxide → 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid methyl ester | HCID 67354675 | — |
| Produkt | 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid | HCID 67356609 | — |
Reaktionsschritte
A solution of 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid methyl ester (100 mg, 0.343 mmol] in 3 ml of mixed solvent [1:0.3:0.5 THF/water/methanol] was treated with lithium hydroxide (12.25 mg, 0.514 mmol]. The reaction mixture was stirred at room temperature for 6 hours, concentrated and acidified [pH=4] with 2M HCl. The precipitate obtained was filtered, washed with water and dried under vacuum. The crude material was washed with ether, air dried overnight to give desired product. i.e., 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid [12] as yellow colored solid. On the basis of mass recovery (93.2 mg) the yield was assumed to be quantitative.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08962637B2 |
| Quelldatensatz | uspto-grants-2015_02 |
| ORD ID | ord-4f29474499c7484c88e9823d1adea9ae |
| Quellennotiz | uspto-grants-2015_02 |